Utilization of petroleum-pitch



K. NOMI. UTILIZATIONOF PETROLE-UM FITCH.

APPLICATION FILED JAN. 22, I9Is.

Patented Aug. 9, 1921a Condensefor,

Heavy 02Z flea/ffll pitch, this is heated graduall UNITED STATES PATENToFFlcl-z.

KONOSUKE NOMI, 0F HTATOSm-GU, JAPAN.

UTILIZATION 0F PETROLEUH-PITGH.

fo all whom itmay concern.'

-Be it known that I, KoNosUKE NOMI, a sub'ect of 'the Emperor of Ja an,residing at 0,-1987 ASugau'ro-Mura, {itatoshimagun, Tokyo Province'Japan, have invented.

heating it tothe temperature of about 500 to 600 C. .to carry outdestructive distillation. The object of this invention is to obtainthese products cheaply.

The petroleum pitch preferably employed ifn the process, is a by-productof refining petroleum oils containi tively large quantities. nThemelting point of the material varies'mor'e or less, depending upon theexact mode of production. A particular samplemelted at 80 C., and thismay be considered as an average melting point.

In carrying this invention into practice, a suitable retort made of castiron or of lire clay is employed. After charging this retort with asuitable quantity of etroleum EVhe'n the charge is heated to about 400(1., (which may require about two hours) it begins slowly to decompose,which operation becomes most eiiicient when the temperature reachesabout 400 to 550 C., say about 500 C. During this operation, apressureof about 4. or 5 poundsper square inch above atmospheric ispreferably maintained in the retort. The mass in the retort is thenheated further,

care being taken that the temperature does not exceed 600 C., thedecomposition into the products labo-ve mentioned is completed. Duringthis latter step, a pressure slightly below atmospheric is used, asuction of 1 to 2 inches being preferred. The retort will contain cokeof the best quality with only a very small percentage of impurities. Thedistillate is collected in a suitable receiver by passing the volatileproducts through a condenser which is connectedto the retort.

The gas is led into a tank through an iron,

Specition of Letters Patent.

olens in rela-` Patented Aug. 9, 1921.

Aliplication mea January 22, isis. seriaims. 213,124.

invention are roughly vgiven in the follow-i ing ltable (per1000.kgs.,of the petroleum pl c v 4 Coke, about 450 kilograms.Distillate, about 250 kilograms. Gas consisting largely of hydrogen;about 6000 cubic feet.

In a particular test run of the process-the products produced wereexamined with the following results:

(a) 'Composition of coke.

H2O 1.74% Volatile part 3.74% Carbon part 92.06% S 1.00% P Trace Ash1.50%

Caloriiic power 8.743 calories. v (b) Composition of gas.-

H r 60.1% 0 1.5% CO 0.9% CO2 0.7% CH4 18.5% Other hydrocarbons 18.3%

(o) Sp. gr. of volatile oil (fraction distilling between 50 C. and 1100.), 0.852.

This liquid consists .largely of olelin hydrocarbons, but contains some(say 3%, more or less) of aromatic hydrocarbons, toluol, benzol, etc.

The coke remaining in the retort contains only a minute quantity ofsulfur and ash so that it has not only a higher caloric power thanordinary coke, but also is very suitable for raw material for smeltingiron, Vor for producing graphite carbon for electric pur- Jose.

l The fdistillate .collected in the receiver contains about 60% ofvolatile oil having boiling point of under 150 0.), w ich,

therefore, is separated 4from the heavier oils by fractionaldistillation, preferably at not greatly exceeding atmospheric pres'-sure. The residualy oil is mixed with about ten times its weight ofmolten pitch. This mixture is thereafter charged into the retort and thedistlling operation is reeated as before, forming the second run. hevolatile oil obtained in this second run consists chieiiy of aromatichydrocarbons, and ,not only can be used as a solvent for rubber,

- fats or the like, but also can re lace petroleum-benzin, or otherwiseemp oyed` as a volatile oil. l

- The gas produced as a by-product in the dry vdistillation will amountto about 6000 'cubic feet by. volume, perI one ton of the pitch. A partof thisgasl can be burned to supply the amount. of heat required for-carrying out this process and, therefore, no exl 'ing to this'invention the distillateis subjected to fractional .distillation toobtain volatile oil, the residue of which operation can be again chargedinto the retort, with more pitch, to produce coke and volatile o-il, andat the same time gas consisting Vchiefly of hydrogen being produced as aby-product.

Therefore, these products, viz, coke, volatile oil and the gas can bevery` cheaply obtained of comparatively good quality.

In the accompanying drawings, which Ashows one example of apparatussuitable for carrying thisinvention into practice, Figure 1 is,adiagrammatic yelevation of an apparatus for heating the petroleum pitchina retort,` together with its connections.

Fig. 2 Ais a diagranunatic elevation, partly in section', of anapparatus for subjecting the distillate to fractional distillation. Fig.3 is laplan View, partly in section, of the r apparatus shown in Fig. 2.

Y. In Fig.' l, 1 1s a retort furnace having for example, threehorizontal retorts 2, each provided with an-exit pipe 3, leading to ahydraulic main 4. 5 isa tank for collect- ,ing gases escaping from theretort. 6 is another tank orreceiver forcollecting the distillate, whichisl condensed in the hydraulic main 4, which acts as a condenser.

In Figs. 2 and 3, 15 is a still for fractional distillatiomwhicli is tobe charged with the distillate fromv tank 6'. .The material in 15 isdistilled by heating the same sufficiently to cause distillation. glflfrthe pressure rises a little above atmospheric, noI particular "harmis done. The? vapor coming from the still is passed through a pipe16,first partially cooled and-condensed in a condenser "1.7, the

condensate being collected in a receiver '18. A second part of the vaporwhich is not condensed `in 17, is passed through a pipe 19,

condensed in the second rcondenser 20 and is.,

collected yin a receiver:l 21'. The condensate is drawn ofi' frointhereceivers andmayvbe mixed with a new charge of petroleum pitch asdescribed. 0r, if desired, thiscondensate .may be returned to thelvstill by a return pipe 22, which may be provided with a cock 23 for thepurpose. AThe volatile'oil, which is not condensed in the tanks 17'. and20, vis

finally condensed in a condenser in 24. 25 is a charging pipe for thestill. 26 is a safety valve.

rlhe steps of the proce may be carried out at about atmosphericpressure.

'I claim: i,

1. The processrherein described, which comprises destructivelydistilling at about" 500 to 600o C. a mixture of petroleum pitch and theheavy components of the oil produced in the destructive distillation ofpetroleum pitch, whereby an oil containing a large lpercentage ofaromatic hydrocarbons, coke and `as are produced.

rocess of producing coke, volatile oil-l and gas containing hydrogen,which com'- prises charging a suitable retort with petroleum pitch, thenheating it up to about 500C' to 600 C., and collecting the products',fractionally distilling the volatile oil obtained,

and mixing the heavierv fraction lthereof with an additional quantity ofthe vpetroleum` pitch, and heating said mixture to about Y50W-to 600 C.,and collecting the products.

In testimony whereof 'I have hereunto set my hand in presence of twosubscribing witnesses.

y KONUSUKE NOMI'. [1.. 8.]

Witnessesz. k f

HENRY B. HITCHCOCK, JoRG BoDHGADJ.

